September / October 2021 NLGI Spokesman

In this issue:…

Serving the Grease Industry Since 1933 - VOL. 85, NO. 4, SEPT./OCT. 2021

4 President’s Podium 10 A Fresh Look at Lithium Complex Greases Part 2: One Possible Path Forward 32 NLGI Interviews Kenneth Hope, PhD Global PAO Technical Services Manager, Chevron Phillips Chemical 42 High-Performance Multiuse (HPM) Grease Column 45 Elastomer Retrospective

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 petro@vanderbiltchemicals.com  www.vanderbiltchemicals.com  (203) 853-1400



(203) 853-1452

Registered and pending trademarks appearing in these materials are those of R.T. Vanderbilt Holding Company, Inc. or its respective wholly owned subsidiaries. For complete listings, please visit this location for trademarks, www.rtvanderbiltholding.com.

VANDERBILT CHEMICALS, LLC CERTIFIED TO ISO 9001:2015 10002461

PRESIDENT: JIM HUNT Tiarco Chemical 1300 Tiarco Dr Dalton, GA 30720 SECRETARY: WAYNE MACKWOOD LANXESS Corporation 565 Coronation Dr West Hill, ON, M1E 2K3, Canada PAST-PRES./ADVISORY: JOE KAPERICK Afton Chemical Corporation 500 Spring St Richmond, VA 23218

VICE PRESIDENT: ANOOP KUMAR Chevron Lubricants 100 Chevron Way Room 71-7334 Richmond, CA 94801 TREASURER: TOM SCHROEDER AXEL Americas, LLC PO Box 12337 N Kansas City, MO 64116 EXECUTIVE DIRECTOR: CRYSTALO’HALLORAN,MBA,CAE NLGI International Headquarters 118 N Conistor Ln., Suite B-281 Liberty, MO 64068

SPOKESMAN

NLGI

OFFICERS

Serving the Grease Industry Since 1933 - VOL. 85, NO. 4, SEPT/OCT. 2021

4

President’s Podium

6

Industry Calendar of Events

6

Welcome New NLGI Members

6

Advertiser’s Index

DIRECTORS BARBARA A. BELLANTI Battenfeld Grease & Oil Corp of New York PO Box 728 1174 Erie Ave N. Tonawanda, NY 14120 BENNY CAO The Lubrizol Corporation 29400 Lakeland Blvd Mail Drop 051E Wickliffe, OH 44092 CHAD CHICHESTER Molykote Lubricants 1801 Larkin Center Drive Midland, MI 48642 CHUCK COE Grease Technology Solutions 35386 Greyfriar Dr Round Hill, VA 20141 JAY COLEMAN Ergon, Inc. PO Box 1639 Jackson, MS 39215 MUIBAT GBADAMOSI Calumet Branded Products, LLC One Purple Ln Porter, TX 77365 MAUREEN HUNTER King Industries, Inc. 1 Science Rd Norwalk, CT 06852

DWAINE G. MORRIS Shell Lubricants 526 S Johnson Dr Odessa, MO 64076 JOHN SANDER Lubrication Engineers, Inc. PO Box 16447 Wichita, KS 67216 GEORGE SANDOR Livent Corporation 2801 Yorkmont Rd Suite 300 Charlotte, NC 28208 SIMONA SHAFTO KoehlerInstrumentCompany,Inc. 85 Corporate Dr Holtsville, NY 11716 JEFF ST. AUBIN AXEL Royal, LLC PO Box 3308 Tulsa, OK 74101 TOM STEIB Italmatch Chemicals 1000 Belt Line St Cleveland, OH 44109 DAVID TURNER CITGO 1293 Eldridge Pkwy Houston, TX 77077 PAT WALSH Texas Refinery Corp One Refinery Pl Ft Worth, TX 76101

TYLER JARK AOCUSA 8015 Paramount Blvd Pico Rivera, CA 90660 MATTHEW MCGINNIS Daubert Chemical Company 4700 S Central Ave Chicago, IL 60638

RAY ZHANG Vanderbilt Chemicals, LLC 30 Winfield St Norwalk, CT 06855

10

Jim Hunt, NLGI President

A Fresh Look at Lithium Complex Greases Part 2: One Possible Path Forward

J. Andrew Waynick, NCH Corporation

32

NLGI Interviews Kenneth Hope, PhD Global PAO Technical Services Manager, Chevron Phillips Chemical

By Mary Moon and Raj Shah

42

High-Performance Multiuse (HPM) Grease Column

45

Elastomer Retrospective

ON THE COVER

Happy Fall!

TECHNICALCOMMITTEE CO-CHAIRS ACADEMIC&RESEARCHGRANTS: CHAD CHICHESTER Molykote Lubricants 1801 Larkin Center Drive Midland, MI 48642

EDUCATION: DAVID TURNER CITGO 1293 Eldridge Pkwy Houston, TX 77077

EDITORIAL REVIEW COMMITTEE CHAIR: Joe Kaperick Afton Chemical Corporation 500 Spring St. Richmond, VA 23218-2158

TECHNICAL EDITOR: Mary Moon, PhD, MBA Presque Isle Innovations LLC 47 Rickert Drive Yardley, PA 19067

Published bi-monthly by NLGI. (ISSN 0027-6782) CRYSTAL O’HALLORAN, Editor NLGI International Headquarters 118 N Conistor Ln, Suite B-281, Liberty, MO 64068 Phone (816) 524-2500 Web site: http://www.nlgi.org - E-mail: nlgi@nlgi.org The NLGI Spokesman is a complimentary publication.

The current issue can be found on the NLGI website.

The NLGI Spokesman is indexed by INIST for the PASCAL database, plus by Engineering Index and Chemical Abstracts Service.

Microfilm copies are available through University Microfilms, Ann Arbor, MI. The NLGI assumes no responsibility for the statements and opinions advanced by contributors to its publications. Views expressed in the editorials are those of the editors and do not necessarily represent the official position of NLGI. Copyright 2018, NLGI. Send e-mail corrections to nlgi@nlgi.org.

-3NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

Jim Hunt NLGI President 2020 – 2022 As part of our ongoing commitment to keep all our NLGI members informed of the status of our six strategic priorities, for this issue, we will focus on effective governance and leadership for NLGI. NLGI’s governance and financial health are critical to the foundation of the organization. I’m happy to report NLGI is financially healthy. In 2020, we ended the year with a net surplus of $80,000, not including the healthy return on our investment account. I’m also pleased to announce that we have exceeded our membership retention goal again this year for the third year in a row! For a year that fell during unprecedented times, the Board of Directors was very pleased with the outcome.

Additionally, NLGI leadership recognizes the need to continuously review our governance structure and evolve as needed. This is extremely important for the long term healthy and sustainability of the organization. Over the next several months, NLGI will review our current structure by honoring the past while focusing on the future. The future changes to the structure of the NLGI is a long term strategy that will take time to implement. We will continue to communicate back to the membership along the way. We appreciate your patience and feedback.

NLGI would like to extend our sincerest gratitude to all the volunteer members that have and continue to provide value to NLGI and our members. These volunteers have offered their skillsets and dedication to ensure that NLGI remains a valued organization. The value of member engagement is never underestimated or unappreciated. NLGI gladly welcomes all volunteers to assist in our committees. These essential committees are truly the engine that keeps NLGI moving forward. Please feel free to contact us at https://www.nlgi.org/about-us/committees/ to indicate which committees align with your interest and talents. Volunteering for NLGI committees provides an excellent opportunity to gain a deeper understanding of the organization’s mission and how to provide value to NLGI members. We invite you to be a part of the decisions made! Contact nlgi@nlgi.org if you’re interested in getting more involved or if you have any questions.

For more information on NLGI’s strategic priorities, I invite you to visit NLGI’s website or read all President’s Podiums from the 2021 Spokesman for more details. Strategic priorities discussed in previous 2021 President’s Podiums include: 1. Membership growth, engagement and global outreach 2. Providing expanded educational opportunities 3. Enhancing opportunities for networking and discussion on emerging industry trends/ applications 4. Certification upgrade – implementation, engagement, marketing Once again, the NLGI is tremendously grateful for your continued support, loyalty, and commitment.

Stay safe and healthy, Jim Hunt President, 2020 – 2022 -4NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

VALVOLINE SERBIAN FACILITY

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For more distance and less downtime, contact us at valvoline.com/en-europe/greases.

TRUSTED FOR 150 YEARS

Industry Calendar of Events 2021 Please contact Denise if there are meetings/conventions you’d like to add to our Industry Calendar, denise@nlgi.org (Your company does not have to be an NLGI membeer to post calendar items.)

October 9-12, 2021

ILMA Annual Meeting

Phoenix, AZ

ILMA Annual Meeting

2021 Machinery Lubrication October 19-21, 2021 Louisville, KY NORIA Machinery Conference & Exhibition Lubrication Conference

& Exhibition 2021 ELGI Autumn Meeting

October 25 - 29, 2021

Amsterdam, Netherlands

2021 ELGI Autumn Meeting

F + L Week Live!

November 15-18, 2021

Bangkok, Thailand

F + L Week Live!

Lubricant Expo

September 6-8, 2022

Messe Essen, Germany

Lubricant Expo

Warm Welcome to our New NLGI Member HYDRAMAQ S.A. Technical

Panama

Advertiser’s Index Afton Chemical Corp, page 7

Daubert Chemical Company, page 41 ELGI, page 56 ERGON, page 57 Harrison Manufacturing, page 33 Hommak Makina Sanayi ve Ticaret A. S., page 9 Kimes Technologies International, Inc., page 39 Lubrication Engineers, Inc, page 37 Patterson Industries Canada - A Division of ALL-WELD COMPANY LIMITED, page 34 ProSys Servo Filling Systems, page 36 Texas Refinery Corp, page 38 The Lubrizol Corporation, page 8 Valvoline, page 5 Vanderbilt Chemicals, LLC, Inside Front Cover Zschimmer & Schwarz Inc., page 35 -6NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

GREASE

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NEW NLGI CLASSIFICATIONS FOR HIGH-PERFORMANCE MULTIUSE (HPM) GREASES ARE HERE.

THAT’S WHERE AFTON’S GREASE MICROBOTZ™ SMOOTH THE WAY. PROTECTING EQUIPMENT AND PROLONGING THE LIFE OF INDISPENSABLE MACHINERY WHERE CONDITIONS ARE AT THEIR HARSHEST. CUSHIONING THE GRIND OF HEAVY LOADS. KEEPING WEAR, CORROSION, AND CONTAMINATION AT BAY. AFTON’S BROAD RANGE OF COMPONENTS AND MULTIFUNCTIONAL GREASE ADDITIVE PACKAGES KEEP GREASE FORMULATING SIMPLE; MAKING COMPLEX, MULTI-INVENTORY MANUFACTURING A THING OF THE PAST, AND GRANTING MAXIMUM FLEXIBILITY FOR PRODUCERS OF SPECIALIZED GREASES. LET AFTON HELP YOU MEET ANY OF THE NEW REQUIREMENTS FOR NLGI’S HIGH-PERFORMANCE MULTIUSE (HPM) GREASE.

www.AftonChemical.com/HPMgrease

© 2021. Afton Chemical Corporation is a wholly owned subsidiary of NewMarket Corporation (NYSE:NEU).

AFTON®, HiTEC®, MicrobotzTM and Passion for Solutions® are trademarks owned by Afton Chemical Corporation. Passion for Solutions® is a registered trademark in the United States.

The Lubrizol Corporation www.lubrizol.com

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Lubrizol offers a wide range of expertise in formulating and manufacturing to ensure product success.

Contact a Lubrizol representative for more information on NLGI HPM.

© 2021 The Lubrizol Corporation. All rights reserved. 21-485

HIGH PRESSURE HOMOGENIZER FOR GREASE APPLICATION

The Brand of

Innovative production

HIGH PRESSURE HOMOGENIZATION IN GREASE PRODUCTION: The homogenization step is very important in grease production. Homogenization not only improves the physical appearance of the grease, but also saves on thickener. In addition, it contributes positively to many performance features such as the pumpability of the grease, mechanical stability, and dropping point. The homogeneous distribution of additives in the grease significantly increases the load carrying and anti-wear capability of the product, allowing you to get better results by using less additives and thickeners.

Suitable for NLGI : 000-3. (Lithium, Lithium complex, Calcium, Calcium Sulphonate Complex, Polyurea, Aluminum Complex, Bentonite, Greases with solid lubricants) Working Pressure : 0-800 Bar (Wide operating range for many grease types from 0 to 800Bar) Operating Temperature : 50 ° C to max. 150 ° C After the saponification step, the remaining oil is added and the mixture is ready to be homogenized.

With High Pressure Homogenization of Grease; Homogeneous distribution of all components in the grease More stable structure and prevention of oil separation More efficient effect of the additive used Quality improvement High NLGI value with effective tightening Prevention of phase separation Improving texture and appearance Crystal and gel structure to obtain a smooth product

Balkan Caddesi No:29 Yazıbaşı / Torbalı - İZMİR

info@hommak.com

www.hommak.com

+90 232 257 54 44

A Fresh Look at Lithium Complex Greases Part 2: One Possible Path Forward J. Andrew Waynick NCH Corporation 2730 Carl Road, Irving, TX

Abstract This paper documents the development of new lithium complex grease technology and provides some insight into why it works the way it does. This new technology involved the addition of a very small amount of overbased magnesium sulfonate (OMgS), overbased calcium sulfonate (OCaS), or both to the initial base oil before adding the thickener acids. Water and lithium hydroxide monohydrate were also added before the thickener acids. When properly used, this approach allowed both thickener acids (longer chain monocarboxylic acid and shorter chain dicarboxylic acid) to be added at essentially the same time with only one heating and cooling cycle. Additionally, the ratio of longer chain monocarboxylic acid to shorter chain dicarboxylic acid could be increased to as much as 5.8. This was in contrast to prior technologies where that ratio was between 1.0 and 3.2. The much higher value of this ratio resulted in a significantly lower required amount of lithium hydroxide monohydrate to achieve grease with the same final consistency. Also, since the cost of the shorter chain dicarboxylic acid was typically 4 to 5 times the cost of the longer chain monocarboxylic acid, further cost reductions resulted.

When using this new technology, the chemical reaction between the lithium hydroxide (LiOH)and the two thickener acids occurred almost instantaneously, in contrast to typical prior art technologies where the reaction required much more time. Greases made using this approach had dropping points typically between 292 C and 328 C. Closed and pressurized reaction vessels or contactors were not required; open reaction vessels could be used to achieve these results. When properly formulated, high performance lithium complex greases with significant cost reductions were possible.

Abbreviations f/m formulation/manufacturing 12-HSA 12-hydroxystearic acid azelaic acid H2Az KOH potassium hydroxide Li lithium LiOH lithium hydroxide LiOH(aq) aqueous solution of lithium hydroxide . lithium hydroxide monohydrate LiOH H2O OCaS overbased calcium sulfonate OMgS overbased magnesium sulfonate PAO poly alpha olefin W/60 Worked 60 stroke penetration value Introduction A review of the development of lithium (Li) complex greases has been provided in the previous Part 1 paper [1], and that information will not be repeated here. However, the important points from that paper will be referred to as appropriate. Therefore, the reader is encouraged to read the Part 1 paper before reading this Part 2 paper.

- 10 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

Over the last ten years, lithium prices have greatly increased, driven primarily by the greater demand for lithium-based batteries.[2] This has resulted in a similar increase in formulation costs for lithium-based lubricating greases. This has been the subject of discussion in previously published papers.[3-5] Three alternatives to this situation have been suggested: (1) use greases with other thickener chemistries that provide similar or improved performance at lower cost; (2) develop new finished lithium-based grease formulations with much higher performance properties, thereby reducing customer grease usage rates and associated cost; (3) develop new lithium-based grease thickener chemistry that will significantly decrease the required amount of lithium (and resulting cost) without reducing the performance.[1] The work documented in this paper falls within the third of these alternatives and was disclosed in a recently issued U.S. Patent.[6] The development objectives for this new lithium-based thickener chemistry were specific for lithium complex greases, but would also be applicable for simple lithium soap greases.

Those development objectives were: • Applicable to open (non-pressurized) vessels.

• Applicable to all types of lithium complex greases.

• Does not require lithium hydroxide (LiOH(aq)); solid lithium hydroxide monohydrate (LiOH.H2O) and water can be added separately.

• Uses thickener acids, not the ester forms (no alcohol formed).

• Thickener acids are 12-hydroxystearic acid (12-HSA) and azelaic acid (H2Az).

• Thickener acids are added at essentially the same time.

• Thickener/acid ratio, 12-HSA/H2Az (wt/wt), is at least 3.2, preferably at least 5.8.

• Only one heating/cooling cycle required during manufacture.

• Provides dropping points of at least 260 C, preferably 300 C. • Compatible with all additives typically used in finished lithium complex greases.

• Provides a potential path to using less lithium for a grease of given consistency and dropping point.

The target values for the thickener/acid ratio, as indicated above, were based on the values reported in the Part 1 paper. The highest thickener/acid ratio reported in that paper was 3.2. The importance of the thickener/acid ratio can be seen by considering the following: Each gram of 12-HSA requires 0.14 grams of LiOH.H2O. Each gram of H2Az requires 0.46 grams of LiOH.H2O. Therefore, H2Az requires just over 3 times as much LiOH.H2O as 12-HSA on a weight/mass basis.

Li 12-HSt is the primary source of thickening; Li2Az is a relatively poor thickener.

Li2Az imparts a higher dropping point but not greater thickening.

Any method that increases the 12-HSA/H2Az (wt/wt) ratio lowers the relative amount of Li2Az and increases the relative amount of Li 12-HSt in the overall thickener.

• This can be expected to lower the cost by at least three ways:

• • • • • •

Ø H2Az requires much more LiOH.H2O than 12-HSA; lowering H2Az lowers the required amount of LiOH.H2O. Less LiOH.H2O lowers the cost. Ø H2Az typically is much more costly than 12-HSA; lowering the required amount of H2Az lowers the cost. Ø When the complex thickener more closely resembles Li 12-HSt, thickener yield can be expected to increase; higher thickener yield lowers cost.

- 11 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

The challenge in increasing the thickener/acid ratio (lowering the relative amount of H2Az) is that such a change would be expected to lower the dropping point. The significance and importance of the dropping point as a true indicator of lubricating grease high temperature performance has been the subject of recent discussion.[7] Certainly, it is possible for a lubricating grease to have a high dropping point yet provide poor high temperature performance. Nonetheless, the dropping point test does provide a tool to determine if changes in lithium complex grease thickener reaction chemistry might be causing a change in structural stability. Additionally, end use customers will likely continue to have dropping point requirements for the foreseeable future. Therefore, it is a reasonable development objective to maintain a typical lithium complex dropping point in any new formulation chemistry.

To achieve the development objectives, including the target thickener/acid ratio and dropping point requirement, a new formulation/manufacturing (f/m) approach was required. This paper describes a new formulation approach that was a significant departure from the previously documented technologies reviewed in the Part 1 paper. It featured a very small amount of an overbased magnesium sulfonate (OMgS) added at the beginning of the process. The TBN value for the OMgS was approximately 400 mg KOH/gram.

Small amounts of water and solid LiOH.H2O were also added at approximately the same time. The thickener acids were added later, after the reaction mixture had been heated. Further details of this new formulation approach are provided in the next section.

Experimental General Grease-Making Procedures, Test Methods, and Raw Materials All greases were made by the same operator using a tilt-head stand-style kitchen mixer with a planetary stirrer and electric heating mantle. All weights were measured using an open pan analytical balance capable of measuring to the nearest 0.01 g. Each grease was given three passes through a three-roll mill with both gaps set at 0.03 mm (0.001 in). The temperature of each grease immediately prior to milling was typically about 66 C. In order to compare the wt% LiOH.H2O of different greases, such comparisons needed to be done on an equal worked penetration basis. However, making greases to an exact predetermined worked penetration is virtually impossible. Therefore, a method was needed to estimate the composition that a grease of given worked penetration would have at a target worked penetration value. The target worked penetration value chosen was 300 (in tenths of a millimeter or points). The method to estimate the wt% LiOH.H2O of a grease at the target penetration value was based on an inverse linear relationship between thickener content (which is linearly related to total lithium content) and worked penetration. This relationship can be stated as follows: wt% LiOH.H2O (W/60 = 300) = W/60 * wt% LiOH.H2O 300 where W/60 is the worked 60 stroke penetration. The values of W/60 and wt% LiOH.H2O in the numerator are the actual values of the grease being considered. While this relationship is not exact, it provides a good estimate as long at the difference between the actual grease penetration value and the target penetration value is less than 30 points. All the greases discussed in this paper meet that requirement.

Additional details concerning each laboratory grease batch were as follows: • All greases used the same paraffinic Group 1 base oil, 113 cSt at 40 C. • All greases were initially formulated to about 14% wt Li-X thickener assuming 100% of the formula base oil was added in the finished grease.

- 12 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

• The initially added portion of base oil was 60 wt% of the total formula base oil amount.

• Water added as reaction solvent was about 0.8 wt% of target finished grease weight.

• Upon cool down from the top temperature, additional base oil was added as needed to allow adequate mixing and achieve an estimated worked penetration between 280 and 300 points for the finished grease.

• The lithium content of greases was measured by wt% LiOH.H2O, even though it was understood that almost all LiOH.H2O had reacted with acids to form thickener salts and that the slight stoichiometric excess was present as anhydrous LiOH. • The wt% LiOH.H2O for all greases was normalized to what it would have been if the greases were at W/60 = 300. This was simply a bookkeeping device for easier comparison of the lithium content of the greases. This normalized value is referred to as the “lithium demand” in this paper.

The primary test methods used to evaluate the greases were dropping point by ASTM D2265 and penetration by ASTM D217. A modified ASTM D2265 procedure was used wherein the block temperature was set at 343 C to apply the same thermal stress to each grease. It should also be noted that ASTM D2265 defines dropping points to values up to 316 C, and the correlation between ASTM D2265 values and real world grease performance is not defined at any temperature. However, in this study, the modified dropping point method was used to detect possible changes in grease structural stability. It was also used, as previously mentioned, to insure that developed lithium complex greases had dropping point values considered acceptable by current industry standards.

A few representative greases were additionally evaluated by the following test methods: • • • • • •

Worked 100,000 stroke penetration, ASTM D217.

Roll Stability at 25 C and 150 C, ASTM D1831.

Oil Separation Properties by Conical Sieve, ASTM D6184.

Copper Strip Corrosion at 100 C and 150 C, ASTM D4048.

Four Ball Wear, ASTM D2266.

Four Ball EP, ASTM D2596.

All raw materials were of a purity typical as is used in the lubricating grease industry. Additionally, calcium carbonate (CaCO3) and anhydrous calcium sulfate (CaSO4) were food grade purity powders with a mean particle size between 1 and 5 microns.

Appropriate safety measures were used during the preparation and testing of all greases in this paper.

The New Formulation Approach for Greases A series of lithium complex greases were made using the new f/m approach as summarized above. Details concerning the manufacturing process of these greases were as follows: 1.

2.

3.

4.

Add the initial base oil, then begin mixing.

Add a small amount of aryl amine antioxidant (0.5 wt% in the final target grease).

Add the 400 TBN OMgS (0.5 wt% in the final target grease) and mix for 15 minutes.

Add the water and all the LiOH.H2O (required for both acids plus about 0.1 wt% excess as anhydrous LiOH).

5. Heat to 82 C – 88 C. 6. Add all the 12-HSA and allow it to melt and visibly react to form the initial grease (which took about 1 minute).

7. Add the H2Az. - 13 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

8. Increase the temperature to 88 C. 9. Let the batch react for 45 minutes.

10. Heat to 204 C to 210 C and hold for 15 minutes.

11. Begin cooling.

12. Add more base oil as needed to maintain adequate mixing.

13. Cool to 77 C, add more base oil as needed, and mill.

This process is depicted below in Figure 1. Note that the time scale on the x-axis is only an approximation.

Certain intentional variations in heating and cooling rates were used for some greases, as will be explained below.

Note that the LiOH is added at the beginning of the process, and that the thickener acids are added later.

This is the opposite of every previous technology discussed in the Part 1 paper. Also note that in accordance with one of the development objectives, there was only one heating and cooling cycle. Additionally, there was no use of esters [8], glycols [9], or a very slow and controlled addition of acids or bases.[10] The Baseline Formulation Approach for Greases In order to evaluate the new f/m approach, comparison greases needed to be made by an approach that was typical of older and well-established technology. Using the information discussed in the Part 1 paper, a baseline formulation and manufacturing process was chosen. Details were as follows: 1. Add the initial base oil, then begin mixing.

2. Add a small amount of aryl amine antioxidant (0.5 wt% in final target grease).

3. Heat to 82 C. 4. Add all the 12-HSA and allow it to melt and mix in. .

5. Add all the LiOH H O (required for both acids plus about 0.06 wt% excess as anhydrous LiOH).

2 6. Increase the temperature to 88 C 7. Add water.

8. Let the batch react for 30 minutes.

9. Heat to 138 C to 143 C. 10. Cool to 88 C and add water.

- 14 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

11. Add the H Az. 2 12. Let the batch react for 30 minutes.

13. Heat to 198 C to 204 C and hold for 15 minutes.

14. Begin cooling.

15. Add more base oil as needed to maintain adequate mixing.

16. Cool to 77 C, add more base oil as needed, and mill.

This baseline f/m process is depicted below in Figure 2. Note that the time scale on the x-axis is only an approximation. Certain intentional variations in heating and cooling rates were used for some greases, as will be explained below.

As can be seen, this baseline f/m approach was essentially the same as a process discussed in the Part 1 paper where each of the two thickener acids was neutralized separately with a heating and cooling cycle between them. Then, a second heating and cooling cycle provided the final co-crystallization of the two thickener salt components.[11] The only difference in this new process from the original older technology was the separate addition of water and all the solid LiOH.H2O instead of the addition of LiOH(aq). This was done so as to make the new f/m and baseline approaches alike in this regard. By doing this, any observed differences in the results of these two approaches could not be attributed to a difference in the initial source of LiOH or how it was added (all at the same time vs. separate additions).

A comparison of the two f/m approaches is summarized in Table 1.

- 15 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

Note that the baseline formulation is color-coded green; the new formulation is color-coded blue. This color coding will be used for the remainder of this paper.

Results And Discussion Initial Evaluation The new f/m approach was initially evaluated by making two greases. Grease 1 was prepared using the baseline approach; Grease 2 was prepared using the new approach. Compositional information and penetration results are provided in Table 2.

Note that certain key results in Table 2 are shown in red font. This is done to help focus attention on the most important information. This convention will be used in the remaining Tables.

The thickener/acid ratio of Grease 1 was 2.89. This value was chosen since it represented a median value from the previous literature as summarized in the Part 1 paper. The thickener/acid ratio of Grease 2 was 3.70. This value was more aggressive (less relative amount of H2Az) than the originally stated minimum development objective of 3.2. The reason for this more aggressive choice was to provide a more severe initial test for the new formulation approach. Since no previously reported lithium complex grease technology had a thickener ratio that high, Grease 2 would serve as a challenging first trial.

The lithium demand for Grease 2 (new f/m) was less than the baseline Grease 1 (older f/m). Examination of the total reacted thickener amount, total LiOH.H2O used, and penetration values provided the reason. Even though Grease 2 was somewhat softer than Grease 1, the total thickener level was also lower in Grease 2.

Grease 2 thickener had a much lower amount of Li2Az due to the higher thickener/acid ratio (less H2Az).

These factors drove the Li demand down in Grease 2 compared to Grease 1.

However, how did this significantly higher thickener/acid ratio (less H2Az) affect dropping point? Figure 3 provides the dropping point results for Greases 1 and 2.

- 16 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

The dropping point of Grease 2 was significantly higher than that of Grease 1. This was so despite the much lower relative amount of H2Az used in Grease 2.

Because of the excellent dropping point results of Grease 2, the shear stability of Greases 1 and 2 were determined using W/100,000 penetration and roll stability run at 25 C and 150 C. Results are given in Figures 4-6.

- 17 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

The shear stabilities of Greases 1 and 2 were the same when determined by W/100,000 penetration (Figure 4). However, when determined by roll stability at 25 C (Figure 5), Grease 2 (new f/m) demonstrated improved shear stability compared to Grease 1 (older f/m). This improvement in shear stability increased when the test was run at 150 C (Figure 6). This is a significant finding since shear stability can be expected to be a function of temperature, just like every other physical and chemical property of matter. The primary reason for using a lithium complex grease instead of a simple lithium soap-thickened grease is to achieve better performance at higher temperatures. Since shear stability is an important grease property, having improved shear stability at higher temperatures is also important, especially when using a grease that is supposed to perform well at higher temperatures.

The above test results suggested that the new f/m approach (Grease 2) differed fundamentally from the older f/m (Grease 1). This was further supported by the striking difference in the appearance and behavior of these two greases during the initial thickener formation reactions. Table 3 summarizes the observations made during thickener formation for Greases 1 and 2.

Clearly, the presence of the small amount of overbased magnesium sulfonate and the addition of acids to base (instead of base to acids) in the new f/m caused a very different reaction dynamic than in the older f/m.

The new f/m caused a very rapid thickener reaction and an equally rapid formation of a grease structure that did not occur when the more traditional older f/m was used. This rapid visible thickener formation was observed for every new f/m grease described in this paper, except where otherwise specified. The significance of this will be explained later in this paper.

- 18 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

All the above observations and interpretations regarding the new f/m approach compared to the baseline approach should be considered correct at least within the process conditions used herein. This caveat will also be understood to be true for all subsequent observations and interpretations for the remaining greases.

Effect of Heating and Cooling Rates The test results and visual behavior during the making of the previous two greases clearly showed a significant difference in the two f/m approaches. However, the time required to heat both greases to their top processing temperature (about 204 C) was about 1.5 hours. Cooling both greases from the top processing temperature to 77 C was accomplished by removing the electric heating mantle and mixing with open air cooling. Cooling to 77 C took approximately one hour. Such heating and cooling rates are significantly faster than what would typically be experienced by commercial batches made in open kettle systems.

As explained in the Part 1 paper, the importance of heating and cooling rates for lithium-based grease thickener structure was understood more than 60 years ago. Accordingly, two greases, Greases 3 and 4, were made using significantly slower heating and cooling rates. The final heating to the top processing temperature took 3 hours; cooling from the top processing temperature to 77 C took 2 hours. These heating and cooling rates were chosen as a compromise: they were closer to commercial open kettle production rates, but still allowed the batches to be made in one day.

Grease 3 was a baseline grease similar to Grease 1. However, the thickener/acid ratio for Grease 3 was increased to 3.71. This was done to bring the relative amount of H2Az in this baseline grease to the same level as the new f/m grease. Grease 4 was a new f/m grease similar to new f/m Grease 2. Grease 4 had a thickener/acid ratio of 3.71, essentially the same value as Grease 2. But like Grease 3, Grease 4 was prepared using slower heating and cooling rates. Thus, Greases 3 and 4 had the same thickener/acid ratio (3.71) and used the same slower heating and cooling rates.

Compositional information and penetration results for Greases 3 and 4 are provided in Table 4. For ease of comparison, information for Greases 1 and 2 are also provided.

- 19 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

Several important insights can be drawn from the information in Table 4. First, a comparison of the two baseline Greases 1 and 3 showed that the lithium demand was higher for Grease 3 than Grease 1. This was despite the fact that Grease 3 used relatively less H2Az compared to Grease 1. Examination of the total reacted thickener content and penetration values for these two greases provided the reason. Grease 3 required more thickener than Grease 1, yet still had a softer penetration. This meant that the thickener yield for Grease 3 was less than Grease 1.

The reason for this decrease in thickener yield makes sense if one remembers the known role of the Li2Az thickener component in a lithium complex grease and the effect of a slower heating and cooling rate. Grease 3 was heated and cooled significantly more slowly than Grease 1. This allowed the Li2Az component to more effectively co-crystallize into the overall lithium complex thickener structure in Grease 3 compared to Grease 1. Since Li2Az is a poor thickener (relative to Li 12-HSt), anything that allows the Li2Az to increasingly impart its effect on the overall thickener structure can be expected to lower the thickener yield.

That is exactly what was apparent in the thickener yields of Greases 1 and 3.

When comparing the two new formulation approach Greases 2 and 4, the same trends were observed. The thickener yield of Grease 4 (slower heating/cooling rate) was less than that of Grease 2 (faster heating/ cooling rate); the lithium demand of Grease 4 was higher than that of Grease 2.

However, a comparison of Greases 3 and 4 showed that the lithium demand of Grease 4 was lower than that of Grease 3, just as the lithium demand of Grease 2 was lower than that of Grease 1. In fact, the lithium demand of Grease 4 was 12% lower than Grease 3, whereas the lithium demand for Grease 2 was 6% lower than Grease 1. Thus, the slower heating and cooling rates of Greases 3 and 4 apparently increased the cocrystallization of Li2Az compared to Greases 1 and 2. Nonetheless, the effect of the new f/m approach to lower lithium demand was increased when the slower heating and cooling rates were used.

The effect of the slower heating/cooling rates on dropping points is provided in Figure 7. For ease of comparison, results of Greases 1 and 2 are also included.

The dropping point of Grease 3 was higher than the dropping point of Grease 1, even though Grease 3 used a lower relative amount of H2Az. The reason for this was the same as previously explained in the trends in lithium demand. The slower heating/cooling rates of Grease 3 compared to Grease 1 allowed the Li2Az to impart its effect on the overall thickener to a greater extent. This resulted in a higher dropping point despite the higher thickener/acid ratio.

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In contrast, the two new f/m Greases 2 and 4 had essentially the same dropping point. Whatever effect the new f/m approach was imparting on the thickener structure of Grease 2, that effect appeared to be maximized with regard to the impact on dropping point. The slower heating/cooling rate effect of Grease 4 did not further enhance the co-crystallization process and the resulting dropping point.

A final observation from Figure 7 was that although the slower heating and cooling rates of baseline Grease 3 improved its dropping point compared to baseline Grease 1, neither grease had a dropping point as high as new f/m Greases 2 and 4. Although the dropping points of all four greases were considered acceptable for a lithium complex grease, the new f/m approach provided an improvement in that test property.

Effect of Overbased Magnesium Sulfonate Concentration The most significant difference between the baseline approach and the new f/m approach was the use of a small amount of OMgS in the initial part of the new f/m process. Three more greases, Greases 5 – 7, were made to verify that the OMgS was the prime factor in the advantageous properties thus far observed in the new f/m approach. All three greases used the same new f/m approach and slower heating/cooling rates of Grease 4. However, Grease 5 used half the concentration of the OMgS in Grease 4. Grease 6 used twice the concentration, and Grease 7 used 20 times the concentration, of the OMgS in Grease 4.

Compositional information and penetration results for Greases 5 – 7 are provided in Table 5. For ease of comparison, information for Greases 3 and 4 are also provided.

The data in Table 5 clearly showed that the OMgS was the prime factor that provided the previously observed effects on thickener yield, dropping point, and lithium demand. When the amount of OMgS was halved (Grease 5), the thickener yield and Li demand were essentially the same as for Grease 4. However, when the amount of OMgS was doubled (Grease 6), the thickener yield decreased and the Li demand increased. When the OMgS was increased by a factor of 20 (Grease 7), no visible grease structure formed.

This was despite the fact that the FTIR spectra taken during the Grease 7 processing showed a very rapid completion of the thickener reactions.

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The dropping points of Greases 3 – 6 are provided in Figure 8.

The dropping point of Grease 7 was not determined since that “grease” was fluid. However, the dropping points of new f/m Greases 4 – 6 were all significantly higher than the baseline Grease 3. Note that all the greases of Figure 8 had the same thickener/acid ratio. Even though Grease 6 had an increase in Li demand due to decreased thickener yield (compared to Greases 4 and 5), it nonetheless had a very high dropping point, similar to the other two new f/m greases.

The Role of the Overbased Magnesium Sulfonate Clearly, the OMgS was responsible for the consistent changes observed in the new f/m approach. But what was its role in affecting those changes, and when did it affect the new formulation process? Two more greases, Greases 8 and 9, were prepared to help answer those questions.

Greases 8 and 9 used the same formulation approach, thickener/acid ratio (3.7), and OMgS (0.5 wt%) as Grease 4. However, each of these two greases differed in one very important way. For every previous new f/m grease, the OMgS was added at the beginning of the process. For Grease 8, the OMgS was also added at the beginning. It was also heated using the same slower heating rate. However, when Grease 8 reached top temperature, the mixing bowl was carefully removed (using heavily insulated mitts), immersed in a large vessel of ice, and manually stirred until the batch temperature reached 116 C. This took only 10 minutes.

For Grease 9, the OMgS was not added at the beginning of the process. Instead, it was not added until the normal slower heating and cooling had occurred and the batch temperature had reached 124 C. Dropping point results for Greases 8 and 9 are provided in Figure 9. For ease of comparison, the results of Greases 3 – 6 are also included.

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As can be seen, the dropping points of Greases 8 and 9 were dramatically decreased compared to Greases 4 – 6. In fact the dropping points of Greases 8 and 9 were almost as low as that of the baseline Grease 3 that did not use the new f/m approach. Obviously, the process changes experienced by Greases 8 and 9 almost eliminated the beneficial effect on dropping point otherwise imparted by the new formulation approach.

In Grease 8, the OMgS was added at the beginning of the process. Like all the greases previously prepared with the new f/m approach, a thick grease structure formed within one minute of the addition of the 12HSA. Grease 8 also experienced the same slower heating rate (with the OMgS present) as the previous new f/m approach Greases 4 – 6 . However, once top temperature was reached, the batch temperature was rapidly quenched to 116 C. This rapid quenching was the only difference between Grease 8 and previous new f/m approach, Greases 4 – 6. Therefore, this single process change had to be the cause of the dramatically lower dropping point.

In Grease 9, the OMgS was not added at the beginning. Therefore, when the thickener acids were added to the batch at 82 C, the overbased magnesium sulfonate was not present. This batch did not form a rapid thick grease structure when the 12-HSA was added. Instead, its thickener structure formed in a manner consistent with the baseline Greases 1 and 3 that used the older technology. Grease 9 experienced the slower heating and slower cooling rates. However, the OMgS was added only after the batch had slowly cooled to 124 C. The dropping point of Grease 9 was the same as Grease 8.

The behavior of these two greases and their dropping points prove several things: • Although the initial presence of the OMgS was the cause of the rapid thickener formation when the 12HSA was added, that rapid thickener formation was not the primary cause of the higher dropping points for the previous new formulation approach greases. If it was, then Grease 8 would have had a dropping point similar to Grease 4.

• The presence of the OMgS in the grease during its cool down from top temperature was responsible for the increased dropping points exhibited in the new formulation approach greases.

• There needed to be sufficient time for the OMgS to affect thickener structure (and the resulting dropping point) during the cool down from top temperature. If the cool down was too rapid (Grease 8), or if the OMgS was not present in the grease until the cool down was mostly completed (Grease 9), most of the benefit to the dropping point was lost.

• When the OMgS was added at the beginning (as per the new formulation approach), the effect of a sufficiently slow cool down from top temperature was more important than the effect of the OMgS concentration on final grease dropping point (Greases 5 and 6).

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Given this new insight, the information discussed thus far concerning all the previous greases allows a possible mechanism to be proposed. This mechanism is consistent with all aspects of the chemistry involved, and it allows a reasonable explanation of how the new f/m approach increases dropping point and decreases Li demand. That proposed mechanism is explained in the following logical sequence of statements: 1.

2.

3.

4.

5.

6.

OMgS is an excellent detergent/dispersant.

OMgS will contain MgCO3 and one or both of MgO and Mg(OH)2.

However, LiOH is a MUCH stronger base than MgO, Mg(OH)2, or MgCO3.

In the new f/m approach, there is FAR more LiOH than OMgS. LiOH is very soluble in water; OMgS and its basic components are not.

By the time the temperature reaches 82 C and the thickener acids are added, the water and LiOH are highly dispersed within the initial base oil.

7. The dispersed water is saturated with the very water-soluble LiOH. 8. The total amount of Mg base is VERY small compared to the amount of LiOH. 9. The thickener acids rapidly react with the LiOH. If they react with LiOH in the saturated dispersed water, the water (at 82 C) rapidly solvates more LiOH from the solid LiOH also dispersed.

10. Thickener reactions occur very rapidly until all the thickener acids are reacted.

11. The OMgS that is present during these thickener reactions disperses the formed Li 12-HSt and Li2Az into the base oil to rapidly form a visible thickener structure.

12. If too much OMgS is initially present, it will begin to excessively disperse the Li-X thickener components in the base oil.

13. At first, this will result in a lower thickener yield and higher required LiOH.H2O. 14. At sufficiently high OMgS concentrations, the Li-X thickener will be so dispersed as to be virtually “soluble” in the base oil, resulting in no grease structure.

15. OMgS increases dropping point by facilitating a more intimate and efficient co-crystallization of the Li 12-HSt and Li2Az, allowing even lower relative levels of H2Az to be used.

16. Any enhancement of co-crystallization that occurs during the rapid initial thickener formation (in the presence of the OMgS) is mostly destroyed in the semi-melted state at top temperature.

17. The enhancement of co-crystallization in the final grease primarily occurs as the semi-melted grease at top temperature is cooled, allowing the thickener fibers to form under the influence of the dispersive OMgS. 18. When the cooling is excessively rapid, or if the OMgS is not added until the grease has cooled, the OMgS does not have enough time to do its job, and the increase in dropping point is mostly lost.

19. Allowing less H2Az to be used, and the resulting increased thickener yield causes less LiOH.H2O to be required.

The Effect of Using Even Less Azelaic Acid The previous new f/m approach greases used a thickener/acid ratio of 3.7. This was slightly higher than the minimum target value of 3.2 as stated in the original development objectives. However, those development objectives also set a thickener/acid ratio target as high as 5.8. This represented a very substantial further decrease in the relative amount of H2Az. To determine if the new f/m approach would continue to provide similar improvements in dropping point and Li demand even at such further reductions in H2Az, Grease 10 was made.

Compositional information and penetration results for Grease 10 is provided in Table 6. For ease of comparison, information for Greases 3 and 4 are also provided.

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Grease 10 had a thickener/acid ratio of 5.8 compared to 3.7 for Greases 3 and 4. The lithium demand for Grease 10 was even lower than Grease 4 when both greases were compared to baseline Grease 3.

Examination of the compositional data showed the reason. The reacted thickener concentration in Grease 10 was the same as Grease 4, and Grease 10 was 10 points softer than Grease 4. However, the much lower amount of H2Az used in Grease 10 resulted in a complex thickener with a greatly reduced amount of Li2Az. This resulted in a reduced level of Li in the Grease 10 complex thickener. This lower level of Li in the Grease 10 complex thickener resulted in a lower overall lithium demand when compared to Greases 3 and 4 The dropping point data for Greases 3, 4, and 10 are provided in Figure 10.

The dropping point of Grease 10 (thickener/acid ratio of 5.8) did decrease compared to Grease 4 (thickener/ acid ratio of 3.7). This was not surprising since much less H2Az was used in Grease 10 compared to Grease 4. However, the Grease 10 dropping point was still excellent. Additionally, even though new f/a approach Grease 10 used much less H2Az than baseline Grease 3, its dropping point was still significantly higher.

This result is very significant since no example can be found in the open literature of a non-borated lithium complex grease with such a high thickener/acid ratio and yet such a high dropping point. Additionally, it is known that when the more traditional methods to make lithium complex greases are used, increasing the thickener/acid ratio to 5.0 can reduce dropping point to around 240 C.[12] Clearly, the new formulation - 25 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

approach provided extremely optimized co-crystallization of the two thickener salts, at least under the conditions used in this development work.

The shear stability of Grease 10 was determined by W/100,000 penetration and roll stability at 25 C and 150 C. Results are provided in Figures 11 – 13, respectively. Baseline Grease 3 is also included for comparison purposes.

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As can be seen, the W/100,000 shear stability of Greases 3 and 10 was within an acceptable range. For the roll stability tests, Grease 10 was similar to Grease 3 when tested at 25 C. When tested at 150 C, Grease 10 was somewhat superior, although both greases were within an acceptable range.

Specificity of Thickener Acid Reactivity As documented in the Part 1 paper, in the previous lithium complex grease technologies lithium hydroxide (in aqueous solution) was added to the thickener acids. The only chemical reactions possible were the acid-base neutralization reactions of the LiOH and the thickener acids. However, in the new formulation approach, the LiOH (as solid LiOH.H2O) was added at the beginning of the process. The thickener acids were added later. When those acids were added, LiOH was not the only base available for potential reaction. The basic moieties in the OMgS were also present. The LiOH was always present in a slightly stoichiometric excess relative to the thickener acids. The level of the basic moieties in the OMgS was much lower than the level of the LiOH. The previously provided explanation of the new f/m approach mechanism assumed that the thickener acids would not significantly react with the OMgS under those conditions. None of the previous greases provided any evidence to the contrary. However, to prove whether this was so, another grease, Grease 10A, was made.

Grease 10A was made the same way as Grease 10 except for one important point: the initially added LiOH. H2O was only 90 wt% of the stoichiometric amount needed to react with the thickener acids. This forced the remaining thickener acids to react with the OMgS basic moieties once the LiOH was consumed.

During the grease making process, Grease 10A initially behaved the same as Grease 10. A thick grease structure formed within one minute of the addition of the 12-HSA. However, Grease 10A appeared to thin out more than Grease 10 as the top processing temperature was approached. This softer consistency was never recovered as Grease 10A was cooled from top temperature. No further oil beyond the initial 60 wt% portion of formula oil was added. This is in contrast to Grease 10 where 92.4 wt% of the formula oil was added.

Compositional information and penetration results for Grease 10A are provided in Table 7. For ease of comparison, information for Grease 10 is also provided.

Since the LiOH was intentionally reduced below its stoichiometric required amount in Grease 10A, the calculated Li demand was not the best indicator of thickener yield for this grease. However, the wt% values of the two thickener acids were. Comparing these values for Grease 10 and 10A showed just how badly the thickener yield was impacted when the amount of LiOH was less than what was needed for complete reaction with the thickener acids.

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This result proved that in the previous new formulation approach greases, the thickener acids did react only with the LiOH. If this had not been the case, similar behavior to Grease 10A would have been observed in the other new f/m greases. Nonetheless, it is interesting to note that the dropping point of Grease 10A was just as high as Grease 10. This result continued to support the mechanism previously provided. The effect of the OMgS on the complex thickener co-crystallization during cool down was in full effect in Grease 10A, just as it had been in Grease 10. Even after reaction with thickener acids, the OMgS apparently provided this beneficial effect.

Application to Fully Formulated Greases All the previous greases were base greases. They contained base oil, thickener, and a very small amount of antioxidant. New formulation approach greases also contained the small amount of OMgS. While the results indicated a very significant benefit in Li demand and dropping point, the real utility of the new formulation approach requires that it provide those benefits in fully formulated greases.

Another grease was made as a representative example of a fully formulated grease. When Grease 10 was made, only a portion was removed from the mixer and milled. The remainder was finished using wellestablished additives and additional base oil as needed to achieve the target penetration range. That final milled grease was Grease 11.

The additives used in Grease 11 were as follows: • Zinc di-alkyl dithiophospate • Zinc di-alkyl dithiocarbamate • Alkenyl borated amide • Acrylate-based copolymer • CaCO3 • Anhydrous CaSO4 With the exception of the alkenyl borated amide, the functional use of each of the additives was well known.

The alkenyl borated amide was not included as a means to further improve the dropping point. The ability of that specific borated additive to provide such improvement was actually known to be poor at best. Given its concentration in Grease 11, it would not have increased dropping point more than 10 C. Other borated additives were available that would have had a much more significant impact on dropping point. The reason the alkenyl borated amide was used was due to it being a good ferrous corrosion (rust) inhibitor.

Compositional information and penetration results for new formulation approach Grease 11 are provided in Table 8.

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The Li demand of Grease 11 was 28% lower than baseline Grease 3. This was despite the fact that baseline Grease 3 had a thickener/acid ratio of 3.7 whereas Grease 11 had a thickener/acid ratio of Grease 5.8. The compositional data showed that the reasons for this greatly reduced Li demand were the improved thickener yield and the lower amount of H2Az used to form the thickener.

Additional test data for Grease 11 are provided in Table 9.

The 6th Edition of the NLGI Lubricating Grease Guide states that the dropping point of lithium complex grease is typically 260+ C.[13] The dropping point of Grease 11 easily met that requirement and was also well within the target objectives as stated at the beginning of this paper. All other test results were similarly good. Once again, the shear stability as measured by roll stability was good at both test temperatures. Of particular interest was the fact that the dropping point was shear stable. Even after running the roll stability test at both temperatures, almost no change in the dropping point was observed.

Effect of Using Overbased Calcium Sulfonate All previous new formulation approach greases used a small initial amount (typically 0.5 wt%) OMgS. Based on the proposed mechanism for this new formulation approach, it was logical to investigate the potential use of an OCaS either alone or in combination with the OMgS. Greases 12 and 13 were prepared to do that. Grease 12 used 0.5 wt% of an OCaS instead of the OMgS. The OCaS had a reported TBN value of about 400 mg KOH/gram. Grease 13 also used 0.50 wt% the same OCaS, but also used 0.15 wt% of the previously used oMgS. All other aspects of the new formulation approach remained unchanged for these two greases.

Like previous Grease 11, Greases 12 and 13 were fully formulated greases. Additives were added near the end of the process as is typically done for finished greases. The additives used were as follows: • • • • • • •

Zinc di-alkyl dithiophospate Zinc di-alkyl dithiocarbamate Sulfurized polyisobutylene Alkenyl borated amide Acrylate-based copolymer CaCO3 Anhydrous CaSO4

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A small amount (about 1%) of a PAO (4 cSt at 100 C) was added at the beginning of the process along with the Group I paraffinic base oil.

Compositional information and penetration results for new formulation approach Greases 12 and 13 are provided in Table 10.

During the grease-making process, both greases behaved the same as the other new f/m greases where a small stoichiometric excess of LiOH.H2O was used. The data in Table 10 showed that the new f/m approach continued to provide acceptable dropping points when OCaS was used instead of OMgS (Grease 12).

A very significant reduction in Li demand was also provided. When the OCaS was augmented with a smaller amount of OMgS (Grease 13), the Li demand increased relative to Grease 12. There was still a Li demand improvement compared to the baseline Grease 3. But that improvement was small compared to the improvement provided by Grease 12. Inspection of the data showed the reason. The combined use of the two overbased sulfonates caused a significant reduction in thickener yield. The higher level of thickener increased the Li content of Grease 13. This increased the Li demand for that grease. Apparently, as the total amount of overbased sulfonates (Ca and Mg) increased, the yield eventually began to decrease. This was previously observed in Grease 6 compared to Grease 4.

Conclusions The results discussed above support the following conclusions: 1. At least within the limited scope of the examples provided and the procedures by which they were made, a new f/m approach has been developed that provides one possible path to make lower-cost lithium complex greases with acceptably high dropping points.

2. This new f/m approach apparently provides this path by facilitating a very intimate and efficient cocrystallization of the lithium complex thickener salts as the grease cools down from top processing temperature.

3. This more intimate and efficient co-crystallization process allows less H2AZ to be used relative to the 12-HSA while still imparting a sufficiently high dropping point. This reduces the Li demand of the resulting greases.

4. This new f/m approach appears to be compatible with additives typically used in current lithiumbased lubricating greases.

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5. This new f/m approach provides potential value when making lithium complex greases in open kettle systems.

6. Additional work should be done and reported to demonstrate how this new f/m technology translates to pilot- and full-scale manufacturing.

Acknowledgement The author gratefully acknowledges the help of Joe Garza during the development of this new technology.

References 1. Waynick, J. A. “A Fresh Look at Lithium Complex Greases Part 1: How Did We Get Here?”; NLGI Spokesman, 85(1), Mar-Apr, 2021.

2. McGuire, Nancy “Lithium’s Changing Landscape”; Tribology & Lubrication Technology, February, 2020, pp 32-39.

3. Fish, Gareth, et. al. “Lubricating Grease Thickeners: How to Navigate your Way through the Lithium Crisis”; NLGI Spokesman, 82(1), March-April, 2018, p 50.

4. Shah, Raj “Lithium ion battery demands and a discussion of lithium supply crisis: How worried should we be?”; NLGI Spokesman, 82(5), November-December, 2018, pp 26.

5. Fathi-Najafi, Mehdi, et. al. “Moving Forward…Can Lubricating Grease Be Produced in a More Efficient Way”; NLGI Spokesman, 82(6), January-February 2019, pp 22-28.

6. Waynick, J. Andrew “Composition and Method of Manufacturing Overbased Sulfonate Modified Lithium Carboxylate Grease”; U.S. Patent No. 10,392,577, 2019.

7. Fish, Gareth “The Dropping Point Test – Time to Drop It?”; NLGI Spokesman, 84(3), July-August, 2020, pp 28-41.

8. Pattendon, Warren C., et. al. “Process for Forming a Grease Containing Metal Salt of Mono and Dicarboxylic Acids”; U.S. Patent No. 2,898,296, 1959.

9. Pattendon, Warren C., et. al. “Lubricating Grease Compositions”; U.S. Patent No. 2,940,930, 1960.

10. Carley, Don A., et. al. “Preparation of High Dropping Point Lithium Complex Soap Grease”; U.S. Patent No. 4,435,299, 1984.

11. Gilani, Syed S. H., et. al. “Grease Thickened with Lithium Soap of Hydroxy Fatty Acid and Lithium Salt of Aliphatic Dicarboxylic Acid”; U.S. Patent No. 3,791,973, 1974.

12. NLGI Lubricating Grease Guide, 6th Edition, p 29, 2015 13. NLGI Lubricating Grease Guide, 6th Edition, p 45, 2015

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NLGI Interviews Kenneth Hope, PhD Global PAO Technical Services Manager Chevron Phillips Chemical The Woodlands, TX

By Mary Moon and Raj Shah

“It’s like stepping onto an escalator and not knowing where you will arrive!” Ken Hope joined the faculty at the University of Houston to manage an NMR Lab. Then he found himself with similar responsibilities at the Chevron Phillips Chemical, where the escalator kept moving from laboratory studies of PAOs to new product development and technical service worldwide.

Ken had a similar experience when he started attending meetings of the local section of the Society of Tribologists and Lubrication Engineers.

That elevator moved through the section board, the national board, and now the presidency of STLE. To learn more about Ken’s journeys, read on!

Education and Career

NLGI: Please tell us a little bit about where you grew up and your education.

KH: I was born in the Panama Canal Zone and moved to

Washington, D.C., when I was very young. My father worked for the government, and we moved around quite a bit, including Maryland and Florida. I went to high school and college at the University of Montevallo in Birmingham, Ala. (Roll Tide!)

NLGI: When did you become interested in science or engineering?

KH: I always had an interest in how mechanical and technical things work, and I really enjoyed chemistry when I was in high school.

My Ph.D. was in physical chemistry at the University of Alabama at Birmingham (UAB), where I researched vitamin A analogs using 2D NMR spectroscopy.

I met my wife, Claudia, at UAB. After we were married, I did a brief post-doc at UAB and then joined the University of Houston (UH), which is what brought us to Texas. I wasn’t born here, but I got here as quick as I could!

NLGI: When did you join Chevron Phillips Chemical?

KH: While I was working at UH, corporate recruiters that would call me and ask me if I could recommend a student who had expertise in NMR. On one of these telephone calls, I mentioned that I didn’t have any students with that expertise who was ready to graduate.

The recruiter asked, “How about you? Are you available for an interview?” One thing led to another, and I found myself in Kingwood, Texas, working for the Chevron Chemical Company.

NLGI: Please give us some background about Chevron Phillips Chemical.

KH: Founded in 2000, Chevron Phillips Chemical is a 50-50 joint venture between Chevron Chemical and then Phillips Petroleum, now Phillips 66.

The companies combined most of their global petrochemical assets into one enterprise.

On my end, I joined from the Chevron Chemical side.

To date, Chevron Phillips Chemical is one of the world’s top producers of olefins and polyolefins and a leading supplier of aromatics, alpha

- 32 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

olefins, styrenics, specialty chemicals, plastic piping and polymer resins.

With approximately 5,000 employees, the company and its affiliates own more than $17 billion in assets, including 31 manufacturing and research facilities in six countries.

amount of time that gyroscope kept spinning on a drop of oil!

Made me wonder what else PAOs could do …

NLGI: What were your first responsibilities?

KH: At Chevron Phillips Chemical, I became responsible for the supervision of solution and solid-state NMR spectrometers as well as other instruments (DSC, TGA, Karl-Fischer titration) and

NLGI: How did your career begin at Chevron Phillips Chemical?

KH: I became involved with the technical side of polyalphaolefins (PAOs) very early in my career with Chevron Phillips Chemical.

PAOs have proved to be very interesting both from a chemical standpoint and with regard to the applications where they are used. This led me to working with lubricants and grease.

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NLGI: What particularly interests you about PAOs?

KH: When I first became aware that our company made a synthetic oil, I was curious.

Makes you wonder why?

What are the reasons that this material is needed? I started looking at the properties and studying it myself in the lab and was really astounded at some of the properties, especially its low temperature properties.

I actually took a small sample and applied some to a plastic gyroscope that I found in a box of Cap’n Crunch® cereal (no kidding). I was amazed at the

- 33 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

laboratory equipment (density, viscosity, bromine index and, and melt index).

My primary duties included serving as the key technical contact to the PAO group and determining microstructure of HDPE (high density

polyethylene), LLDPE (linear low density polyethylene) and other methyl and butyl acrylate specialty polymers. I also worked on determining the structures of potential catalyst ligands and performing thermal analyses of high viscosity polyalphaolefins.

DESIGNERS & MANUFACTURERS OF

PROCESS KETTLES FOR THE PRODUCTION OF INDUSTRIAL GREASES

NLGI: What happened next?

KH: In 1997, I became the polyalphaolefin technology manager (1997 to 2000). I lead a technical team that was responsible for developing products and processes for PAOs. There was a major shift from the laboratory to managing the technical developments and interacting with customers but it allowed me to learn more about what was needed for the end applications.

Several inventions I’ve contributed to were commercialized and led to improvements in production, product quality and catalyst efficiency. We invented and commercialized processes for improving the oxidative stability properties of PAOs. I also worked on teams to develop and commercialized PAO 25, Synfluid® mPAO 40 and mPAO 100.

NLGI: What are PAOs and mPAOs?

PATTERSON INDUSTRIES

CANADA

"The Process Equipment People"

A D i v i s i o n o f A L L - W E L D C O M P A N Y L I M I T E D • Engineers Since 1920 49 PASSMORE AVE • SCARBOROUGH (TORONTO), ONTARIO M1V 4T1 • TEL: (416) 694-3381 • FAX: (416) 691 2768 E-MAIL: process@pattersonindustries.com • WEB: www.pattersonindustries.com

KH: PAOs and mPAOs are synthesized from alpha-olefin molecules and distilled and hydrogenated to form highly branched isoparaffins. These are designed to be of a certain molecular weight which will dictate their viscosity. Each are made with specific catalysts to tailor their properties.

In contrast to mineral oils, PAOs are relatively pure. They do not contain unsaturated and ring-type hydrocarbons, sulfur,

- 34 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

nitrogen, and light volatile and heavy waxy hydrocarbons, all of which limit their application in lubricating oils and greases in one way or another. PAOs are noted for their lubricity, high viscosity index, thermal and oxidative stability, fluidity at low temperatures and low volatility at high temperatures.

KH: I’m responsible for providing technical service to current and prospective customers to enhance current sales, margins and develop new PAO opportunities through technical development calls, fielding inquiries, developing new PAO data and participating

in industry advisory boards that define lubricant standards.

I work with colleagues in PAO business management, product management and sales to developed annual technical plans. And I’m responsible for executing projects to increase sales of conventional PAOs and

The fundamental differences between PAOs and mPAOs (metallocene catalyzed PAOs with higher viscosities than most PAOs) are the catalysts that are used to make them and the available viscosity grades.

NLGI: Do you currently spend most of your time working at the bench in the laboratory?

KH: These days, I actually spend a lot of my time travelling and communicating.

I meet with customers and lubricant formulators at key accounts worldwide and explain the benefits of PAOs and mPAOs. I also train distributors in the U.S., South America, Europe, China and South Korea about technical sales of PAOs and mPAOs.

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And I give webinars on PAOs and mPAOs and presentations at the Commercial Marketing Forum at STLE Annual Meetings and NLGI as well as many other industrial conferences.

NLGI: What are your responsibilities at Chevron Phillips Chemical?

Chemistry tailor-made

- 35 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

mPAOs into higher margin, higher value applications.

NLGI: What about patents?

KH: I have 21 so far (and counting.) Many of my patents cover catalysts and processes to synthesize PAOs and prepare lubricants.

NLGI: What particular challenges have you faced during the COVID-19 pandemic and how have you addressed them?

KH: Some challenges are technical and those can be fun and interesting. Some have reminded me of reading

Ken (center) received a medal in recognition of his 20th U.S. Patent. In this photo, he is standing with former President and CEO Dr. Mark Lashier (right) and Senior Vice-President of Technology Don Lycette (left).

a detective novel, and others seem more like whodunnits. At the end of the day, it is always best to keep a teamwork approach and stay positive.

The biggest challenge I had during COVID-19 was a very serious health situation that made it painful to walk or even stand after a few minutes.

Two surgeries, a great deal of physical therapy and four series of injections left me with two options. One, I could have electrodes implanted and a 50/50 chance that they would block the pain or make it worse. Two, I could live with it.

Servo Filling Systems

EST. 1985

After nearly two years of dealing with it, I chose option three and took it to God through prayer asking Jesus to “grow it back.” Two weeks later, I was walking a mile, then further. As I write this, about two months after that prayer, I am able to do whatever I want!

Going from standing or walking for less than 25 minutes to hours on end is hard to explain.

- 36 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

All I can say is that I believe that He healed me. By the way, He healed more than that too and I have the lab reports to document my condition, before and after, with no medical explanation as to why it improved. This is the truth, and I leave it to the reader to grapple with my story.

Ken gave a presentation about the PAO Blending Matrix and mPAO Grease Advantages at the 2019 UNITI Congress.

UNITI is a German association of producers of lubricants and additives and companies in the energy sector.

Grease Industry

NLGI: What do you think about the position and future of the global lubricating grease industry?

KH: The future seems very bright for the grease industry in my opinion. Areas that are so much in vogue now seems to bode well for the grease industry, like electric vehicles for instance.

NLGI: Which new or future applications (e.g., EVs or electric vehicles) show particular promise for affecting the grease industry?

KH: Seems to me that some smart people have already figured out how to deal with the lubrication of electric motors. The number and breadth of applications is increasing and that will be a good thing.

NLGI

NLGI: When and how did you become active in NLGI?

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- 37 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

KH: I’ve attended NLGI meetings over the years, especially since we began producing high viscosity mPAO. The application for that into grease became very interesting and we reached out to our friend Paul A. Bessette, president of Triboscience & Engineering, Inc. We discussed formulating greases with mPAO, and that discussion led to a number of joint projects and presentations at NLGI and ELGI meetings from 2016 to 2019.

NLGI: Why do you attend NLGI Meetings?

KH: Naturally, my colleagues and I attend to interact with customers as well as keep abreast of the latest developments in grease technologies. I feel blessed that over the years I’ve made many friends through NLGI.

NLGI: Do you have favorite memories of NLGI Meetings?

KH: I have very memorable experiences of NLGI Meetings at The Breakers in Palm Beach and Bonita Springs, Fla., at Scottsdale, Ariz., Hot Springs, Va. (and the scenic drive there), Coeur D’Alene, ID, Las Vegas and Williamsburg, Va.! NLGI always picks wonderful venues for meetings.

On the golf course at the 2018 NLGI Meeting at Coeur D’Alene, ID(from left to right): Ramnath Kuthoore (The Lubrizol Corporation), Jared Morgan (Chevron Phillips Chemical), Ken Hope (Chevron Phillips), and Joe Sankovic (Shamrock Technologies)

CELEBRATING OUR 99TH ANNIVERSARY!

TEXAS REFINERY CORP

STLE NLGI: How did you become involved with STLE? What roles have you held?

KH: I became involved because someone suggested I attend a local STLE meeting! This is key — we often forget that we can make a positive difference in someone’s career simply by inviting them into an organization.

Shortly after I started attending local and annual STLE meetings, I was asked to be the editor of the Lube Guide for the Houston Section. Little did I know that this also meant that I had entered the yearly rotation through all of the officer roles and eventually, section chair.

That experience was like stepping onto an escalator but not knowing where I would arrive!

Shortly after reaching the coveted position of past-section chair, Rob Heverly asked if I was interested in serving on the STLE board of directors as regional vice-president. That led to 10 years on the BOD (two two-year terms as RVP and then two 3-year terms as a director). At that point, I waved goodbye and gave my speech thanking the BOD for many great memories.

A few months later, STLE asked me to return to the BOD as treasurer. So I stepped back on the elevator because this was

- 38 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

a five-year commitment through the executive committee to become president.

When I describe this path, it sounds like it took a long time, but it really didn’t seem that long at all. Along the way I have enjoyed so many good times with good friends and challenges too!

These experiences are the things that give flavor to our lives.

NLGI: What are some learnings from being involved on the board of STLE?

KH: I have learned so much from my co-workers on the STLE BOD and the staff as well. These are great people. One thing I learned from Ed Salek, STLE’s executive director is his motto “Work hard. Be nice.” That is a wonderful motto.

It is also so very important to remember for a volunteer organization like STLE or NLGI, a good deal of work gets done by people who aren’t paid to do it. The long history of successes of both organizations is really quite amazing! Our successes today are based upon the hard work of volunteers that did much heavy lifting before us. As you read this, is there something you feel energized to help with?

Ken gave a demonstration to school children on how to make smoky soap bubbles with dry ice during Camp Chemisphere at Chevron Phillips Chemical’s headquarters in The Woodlands,Texas

KH: We enjoy games. We play games almost every day. My wife’s favorite is Parcheesi, but the rules she learned growing up in Colombia are much different than the ones I learned (and are printed on the instructions for that matter – she is going to get me for writing this!). I’m not very good at this version and have been banned from games a couple of times, but I’m getting better.

We also learned a lot of good games during our time in the Czech Republic teaching English at

Perspectives

NLGI: Do you have time to be involved in other volunteer activities?

KH: Chevron Phillips Chemical has been very encouraging and urging employees to volunteer and care for our community. I‘ve been able to participate in a reading program at a local elementary school, science fair judging, Habitat for Humanity projects, United Way Days of Caring and other ways to make a difference.

These activities have all been fun and positive experiences. They are consistent with our company’s tagline “Performance by design. Caring by choice.™” NLGI: What kinds of activities do you and your family enjoy?

- 39 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

a Christian Family Camp. At night after all of the events, we would play “Bang!” and “Love Letter,” where you try through deductive reasoning to get a letter to the princess.

You would think that I’d be able to speak Czech from all of the activities but that would be wrong – it’s a very difficult language but the people we met there are wonderful.

NLGI: If NLGI members travel to Texas, do you have any suggestions?

KH: Don’t come during the summer! You may have heard a rumor that Houston is hot!

The one secret that most people don’t know is that the late winter and early spring are really good times to visit.

When the rest of the country is very cold, it is usually great weather in Houston (unless there is another Texas Snowmageddon!).

As for things to eat, after living in Houston for 33 years, you would think I’d be tired of the bar-b-que, but you’d be wrong.

Texas bar-b-que is great, and there are so many good places to get it. Tex-Mex food is also wonderful especially in San Antonio.

This interview series, started in 2019 by Dr. Moon and Dr. Shah, gives NLGI members a bit of insight into the professional and personal lives of their colleagues, developments in the grease industry, and the

Ken with his daughters Sabrina and Claudia, son Steven, and wife Natalie (from left to right) at Steven’s graduation from the University of Texas at San Antonio (UTSA) with a degree in Mechanical Engineering in 2019

role of NLGI worldwide. If you would like to suggest the name of a colleague for an interview (or volunteer to be considered as a candidate), please kindly email Mary at mmmoon@ ix.netcom.com or Raj at rshah@ koehlerinstrument.com.

Dr. Mary Moon is Technical Editor of The NLGI Spokesman.

She writes scientific and marketing features published in Lubes’n’Greases and Tribology & Lubrication Technology magazines, book chapters, specifications, and other literature. Her experience in the lubricant and specialty chemicals industries includes R&D, project management, and applications of tribology and electrochemistry. She served as Section Chair of the Philadelphia Section of STLE. Dr. Raj Shah is currently a Director at Koehler Instrument Company and was an NLGI board member from 2000 to 2017. A Ph.D in Chemical Engineering from Penn State

University and a Fellow from the Chartered Management Institute, London, Dr. Shah is a recipient of the Bellanti Sr. memorial award from NLGI. He is an elected fellow of NLGI, IChemE, STLE, INSTMC, AIC, KHI, Energy Institute and the Royal Society of Chemistry. A Chartered Petroleum Engineer from EI and a Chartered Chemical Engineer from IChemE, he is currently active on the board of STLE and on the advisory boards of the Engineering Departments at SUNY Stony Brook, Hofstra University, Auburn University and Pennsylvania State University. More information on Raj can be found at https:// www.astm.org/DIGITAL_ LIBRARY/MNL/SOURCE_ PAGES/MNL37-2ND_foreword. pdf

- 40 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

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High-Performance Multiuse (HPM) Grease Column HPM and End-User Promotion Educating end-users on the quality of products using NLGI’s High-Performance Multiuse Grease (HPM) is critical. In December 2020, NLGI launched a HPM Marketing Taskforce to oversee exposure and targeted communications to the end-user audience. To date, more than 600,000 end-users have been reached.

Marketing efforts will continue through the end of 2021 and into 2022.

END-USER PROMOTIONS TO DATE: F&L Asia

EU Lube Magazine

Efficient Plant

August issue of Plant Engineering ran “How the NLGI HPM specification facilitates grease selection”

by Dr. Gareth Fish.

EU Lube Magazine

F&L Asia published an article around NLGI’s press release: “Castrol launches first NLGI Certified HPM Grease in the market” in July 2021.

Efficient Plant article, paired with podcast

Plant Engineering

Pumps & Systems

Machinery Lubrication

Pumps & Systems’ August article on the benefits o f HPM grease certification by Greg Morris, paired with an advertisement.

Machinery Lubrication (NORIA) published, “Multipurpose Does Not Mean All-purpose”

by Wes Cash, Noria Corporation in August.

STLE

NLGI India Chapter

STLE ran a cover story in TLT (September) which highlighted HPM grease spec

Webinar for NLGI’s India Chapter, by Joe Kaperick

ALIA

Webinar for Asian Lubricants Industry Association highlighting HPM, by Joe Kaperick and Chuck Coe

NLGI

HPM series on specification details (must be an NLGI member to access)

Social Media

Continuous social media posts in various industrial manufacturing, chemical and construction sectors.

FUTURE PROMOTIONS INCLUDE: Efficient Plant - Ads in September and November digital newsletter

Pumps & Systems - Ads in September, October and November issues

Construction Business Owner - Ads in September, October and November issues Plant/Maintenance - Direct e-mail campaign to 5,600 end-users

Social Media - Sponsored LinkedIn advertisement to enhance visibility

- 42 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

HPM Marketing Taskforce and CQ have reached overA 1 Million end-user s to date!

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NLGI

ADVERTISE WITH NLGI

The NLGI Spokesman Magazine is published bi-monthly (6 issues per year) in digital format only.

CIRCULATION INFORMATION The NLGI Spokesman is a trade publication sponsored by the National Lubricating Grease Institute. The circulation reaches over 45 countries worldwide.

CLICK HERE to download The Spokesman rate card.

CLICK HERE to download the nlgi.org website advertsing rate card.

Inquiries and production materials should be sent to Denise Roberts at NLGI (denise@nlgi.org)

2021 NLGI Digital Spokesma

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ADVERTISING RATES

The NLGI Spokesman Magazine is published bi-monthly (6 issues per year) in digital format only.

2019 Spokesman Advertising

CIRCULATION INFORMAT ION The NLGI Spokesman is a trade publication sponsored by the National Lubricating Grease Institute. The circulation reaches over 45 countries worldwide.

READERSHIP Manufacturers, suppliers, marketers, distributors, technicians, formulators, scientists, engineers and consumers of lubricating greases.

ADVERTISING DEADLINE S January/February ................... Janueary 11 March/April ....................................March 1 May/June ..........................................

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CONTACT Inquiries and production materials should be to Denise Roberts at NLGI (denise@nlgi.o sent rg)

- 43 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

VERTICAL

SPOKESMAN

NLGI

READERSHIP Manufacturers, suppliers, marketers, distributors, technicians, formulators, scientists, engineers and consumers of lubricating greases.

Check out the NLGI Store Click the sections below to learn more.

nlgi.org/store

NLGI RESEARCH GRANT REPORTS

Grease Lubrication of New Materials for Bearing in EV Motors 2019 - University of California – Merced

Strategies for Optimizing Greases to Mitigate Fretting Wear 2018 - The University of Akron

Determination of Grease Life in Bearings via Entropy 2017 - Louisiana State University

Summary & Full Reports Available

Available to Members Only

Login to the members’ only area to read the report today: https://www.nlgi.org/my-account/

- 44 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

Elastomer Retrospective NLGI’s new series of High Performance Multiuse (HPM) Grease Specifications has now been introduced with a core specification defined (HPM) along with enhanced performance categories for High Load (HL), Low Temperature (LT), Corrosion Resistance (CR) and Water Resistance (WR). Elastomer compatibility was addressed in the core HPM specification with a switch away from the materials (NBR and CR) used in the GC and LB specifications. These materials are described by the Society of Automotive Engineer’s (SAE) Specification AMS 3217/2C (NBR-L) and AMS 3217/3B (CR) and any changes in these materials are under SAE’s control. The material specified in NLGI’s new HPM core specification is the more readily available SRE-NBR 28/P or SRE-NBR 28/PX elastomer as described in ISO 13226.

With this in mind, NLGI would like to highlight the work done by Tom Verdura of General Motors to investigate various methods of looking at elastomer compatibility which was done at the same time as development work around the ASTM D4289 elastomer compatibility test method. We offer a reprint of a Spokesman article from 1978 by T. M. Verdura, “Evaluating Compatibility of Greases with Elastomeric Seals”.

- 45 NLGI Spokesman | VOLUME 85, NUMBER 3 | July/August 2021

- 49 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

- 51 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

- 53 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

- 55 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

GREASE GUIDE (7 EDITION) TH

CO

M

CHAPTERS: • Introduction/Historical Development

IN

G

IN

20

22

• Characteristics of Grease • Grease Testing • Formulation H New Chapter H • Grease Manufacturing • Greases of incidental Food Contact H New Chapter H • Grease Handling • Grease Selection • Grease Troubleshooting • NLGI Certifications H New Chapter H

• Environmentally Acceptable Greases H New Chapter H • Grease HS&E Contact nlgi@nlgi.org with any questions.

Autumn Events 2021 Save the dates 25th - 29th October 2021 Amsterdam Working Group Meetings 25th October 2021 Grease Training Course 26th & 27th October 2021 ELGI-STLE Tribology Exchange Workshop 28th & 29th October 2021 ELGI, Hemonylaan 26, 1074 BJ Amsterdam, Netherlands Telephone: +31 20 67 16 162 I Email: carol@elgi.demon.nl

I

Online: www.elgi.org

- 56 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021

!

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North & South America +1 601 933 3000 Europe, Middle East, Africa + 32 2 351 23 75 Asia + 65 6808 1547

ergonnsa.com - 57 NLGI Spokesman | VOLUME 85, NUMBER 4 | September/October 2021